CN110054489A - A kind of high amplitude magnetic conductivity MnZn Ferrite Material and preparation method thereof - Google Patents
A kind of high amplitude magnetic conductivity MnZn Ferrite Material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to Ferrite Material field, a kind of high amplitude magnetic conductivity MnZn Ferrite Material and preparation method thereof is disclosed.The high amplitude magnetic conductivity MnZn Ferrite Material is by Fe2O3, ZnO and MnO2The principal component and CaCO of composition3、Bi2O3It is constituted with the additive of rare earth oxide composition.Preburning material is made in ball milling, 860~950 DEG C of pre-burnings after principal component is mixed；Then additive mixing, ball milling is added, adds poly-vinyl alcohol solution granulation, granulation material is poured into compression moulding in mold and obtains green body, then heats to 1300~1400 DEG C of sintering, cooling obtains high amplitude magnetic conductivity MnZn Ferrite Material.MnZn Ferrite Material of the invention has high amplitude permeability characteristics.New material selection can be provided for applications such as lower applying frequency (30kHz and following), modest magnetic fields.
Description
Technical field
The invention belongs to Ferrite Material fields, and in particular to a kind of high amplitude magnetic conductivity MnZn Ferrite Material and its system
Preparation Method.
Background technique
As a kind of important functional material, magnetic material has in fields such as household electrical appliances, communication, computer, national defense industry
It is widely applied, yield and usage amount represent the development level of a national economy and information technology.Manganese-zinc ferrite is
It is a kind of very important magnetic material, is that current production rate is maximum, a kind of most widely used typical soft magnetic ferrite, because
It is widely used in various core materials with high magnetic conductivity, low coercivity and low power loss.According to manganese-zinc ferrite
The application characteristic of body can substantially be classified as three categories: high permeability MnZn ferrite, manganese-zinc power ferrite and anti-electromagnetism
Interfere manganese-zinc ferrite.High permeability MnZn ferrite can also be subdivided into high-permeability material (initial permeability be greater than 5000) and
Superhigh magnetic conductivity material (initial permeability is greater than 10000).In different application fields, requirement ferritic for MnZn is very much not
Identical, there may be greatest differences for every magnetic parameter of MnZn.
Summary of the invention
To adapt to the different requirements ferritic to MnZn of different application field, the primary purpose of the present invention is that providing one kind
High amplitude magnetic conductivity MnZn Ferrite Material.It can be the applied fields such as lower applying frequency (30kHz and following), modest magnetic field
It closes and new material selection is provided.
Another object of the present invention is to provide the preparation methods of above-mentioned high amplitude magnetic conductivity MnZn Ferrite Material.
The object of the invention is achieved through the following technical solutions:
A kind of high amplitude magnetic conductivity MnZn Ferrite Material, by Fe2O3, ZnO and MnO2The principal component and CaCO of composition3、
Bi2O3It is constituted with the additive of rare earth oxide composition.
Preferably, the rare earth oxide is Sm2O3。
Preferably, the principal component is made of the raw material of following molar percentage: Fe2O350.5~53.5mol%, ZnO
10~14mol%, MnO232~35.5mol%, the sum of three component molar percentages are 100%.
Preferably, the content of the additive is as follows: CaCO3100~1000ppm, Bi2O3100~1000ppm, rare earth
100~1000ppm of oxide.
The preparation method of above-mentioned high amplitude magnetic conductivity MnZn Ferrite Material, including following preparation step:
A) ingredient: by principal component Fe2O3, ZnO and MnO2It carries out ingredient and is uniformly mixed to obtain mixture；
B) a ball milling: a ball milling material is obtained within ball-milling treatment 2~3 hours after mixture, steel ball and water are mixed；
C) pre-burning: pre-burning after a ball milling material is dried, calcined temperature are 860~950 DEG C, and burn-in time is 1.5~4 small
When, Preburning material is made；
D) secondary ball milling: by addition of C aCO3、Bi2O3It is mixed to get doping material with rare earth oxide and Preburning material, will be mixed
Miscellaneous material, steel ball carry out secondary ball milling after mixing with water, the secondary ball milling time 3~5 hours, secondary ball abrasive material is made after dry；
E) it is granulated: poly-vinyl alcohol solution being added in secondary ball abrasive material, grinding is granulated or mist projection granulating, screened to obtain
100~250 μm of granulation material；
F) it forms: granulation material uniformly being poured into compression moulding in mold and obtains green body；
G) it is sintered: by green body by room temperature to 1300~1400 DEG C of sintering temperature, 3~6 hours is kept the temperature, later by green body
It is cooled to room temperature, obtains high amplitude magnetic conductivity MnZn Ferrite Material.
Preferably, in the step b), when ball milling, mixture and water, steel ball quality ratio are 1:(0.9~1.1): (3~
6)。
Preferably, in the step d), when ball milling, doping material is 1:(0.9~1.1 with water, steel ball quality ratio): (3~
5)。
Preferably, the mass concentration of poly-vinyl alcohol solution is 8%~15%, poly-vinyl alcohol solution in the step e)
Additional amount be secondary ball abrasive material weight 8%~12%.
Preferably, the pressure of compression moulding is 100~200Mpa, 20~60s of dwell time in the step f).
Preferably, the temperature rise period for rising to 1100 DEG C from room temperature is air atmosphere, 1100 DEG C of beginnings in the step g)
It is passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is no more than 5%, and be passed through oxygen-nitrogen mixture body to the holding stage always to terminate, cooled down
Stage is passed through pure nitrogen gas.
Ferrite Material of the invention have the following advantages that and the utility model has the advantages that
MnZn Ferrite Material of the invention has high amplitude permeability characteristics.Can for lower applying frequency (30kHz and with
Under), the applications such as modest magnetic field new material selection is provided.
Detailed description of the invention
Fig. 1 is sample amplitude permeability obtained by embodiment under 100mT and comparative example with the variation relation figure of frequency；
Fig. 2 is sample amplitude permeability obtained by embodiment under 200mT and comparative example with the variation relation figure of frequency.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3300ppm, Sm2O3100ppm,
Bi2O3300ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 1 sample.
Embodiment 2
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3500ppm, Sm2O3100ppm,
Bi2O3500ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 2 samples.
Embodiment 3
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3100ppm, Sm2O3300ppm,
Bi2O3300ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 3 samples.
Embodiment 4
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3300ppm, Sm2O3300ppm,
Bi2O3500ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 4 samples.
Embodiment 5
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3300ppm, Sm2O3500ppm,
Bi2O3300ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 5 samples.
Embodiment 6
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, CaCO is added toward Preburning material3100ppm, Sm2O3500ppm,
Bi2O3500ppm carries out secondary ball milling after mixing, and Ball-milling Time 4 hours, doping material was 1:1 with water, steel ball quality ratio:
4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% poly-vinyl alcohol solution, grinding sieve
Get 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, dwell time 30s.By base
Body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in 1350 DEG C of heat preservation 3h, from room
The temperature rise period of temperature rise to 1100 DEG C is air atmosphere, and 1100 DEG C start to be passed through the oxygen-nitrogen mixture body that partial pressure of oxygen is 4%, and one
Leading directly to terminates into oxygen-nitrogen mixture body to the holding stage；Heat preservation terminates, and is cooled to room temperature with furnace, this stage is passed through pure nitrogen gas,
Finally obtain manganese-zinc ferrite.This sample is denoted as No. 6 samples.
Comparative example 1
Principal component is pressed into Fe2O3, ZnO and MnO2Molar ratio be that 52.5:12:35.5 ingredient and be uniformly mixed, then
Ball-milling treatment 2 hours, mixture and water, steel ball quality ratio were 1:1:4.Pre-burning after ball milling material is dried, calcined temperature are
920 DEG C, burn-in time is 2 hours.After pre-burning terminates cooling, secondary ball milling is carried out, Ball-milling Time 4 hours, doping was expected and water, steel
Ball mass ratio is 1:1:4.Secondary ball abrasive material is made after drying, the concentration that secondary ball abrasive material weight 10% is added is 10% polyethylene
Alcoholic solution, grinding screening obtain 100~250 μm of granulation material.By granulation material compression moulding, briquetting pressure 125Mpa, pressure maintaining
Time is 30s.Green body is put into high-temperature atmosphere tube furnace and is sintered, by room temperature to 1350 DEG C of sintering temperature, in
1350 DEG C of heat preservation 3h, the temperature rise period for rising to 1100 DEG C from room temperature are air atmosphere, and 1100 DEG C start to be passed through partial pressure of oxygen to be 4%
Oxygen-nitrogen mixture body, and be passed through oxygen-nitrogen mixture body to the holding stage always and terminate；Heat preservation terminates, and is cooled to room temperature with furnace,
This stage is passed through pure nitrogen gas, finally obtains manganese-zinc ferrite.This sample is denoted as No. 7 samples.
Sample obtained by above embodiments is tested for the property, soft magnetism alternating-current measuring device MATS- is used at 25 DEG C of room temperature
2010SA carries out test acquirement, and test parameter is set as 10~100kHz of frequency, magnetic induction intensity 100mT or 200mT.Frequency
Sample amplitude permeability result is as shown in table 1 below under 25kHz:
Sample amplitude permeability under 1 frequency 25kHz of table
| Sample number into spectrum | Sample amplitude permeability under 100mT | Sample amplitude permeability under 200mT |
| 1 | 4712 | 5175 |
| 2 | 4822 | 5303 |
| 3 | 4343 | 4847 |
| 4 | 5151 | 5664 |
| 5 | 5004 | 5665 |
| 6 | 5211 | 5930 |
| 7 | 3585 | 3952 |
Sample amplitude permeability is as depicted in figs. 1 and 2 with the variation relation difference of frequency under 100mT and 200mT.
By above-mentioned the performance test results, it can be concluded that, Ferrite Material produced by the present invention has higher compared with comparative example
Amplitude permeability.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of high amplitude magnetic conductivity MnZn Ferrite Material, it is characterised in that: the high amplitude magnetic conductivity MnZn ferrite material
Material is by Fe2O3, ZnO and MnO2The principal component and CaCO of composition3、Bi2O3It is constituted with the additive of rare earth oxide composition.
2. a kind of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 1, it is characterised in that: the rare earth
Oxide is Sm2O3。
3. a kind of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 1 or 2, it is characterised in that it is described it is main at
Divide and be made of the raw material of following molar percentage: Fe2O350.5~53.5mol%, ZnO 10~14mol%, MnO232~
35.5mol%, the sum of three component molar percentages are 100%.
4. a kind of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 1 or 2, it is characterised in that the addition
The content of agent is as follows: CaCO3100~1000ppm, Bi2O3100~1000ppm, 100~1000ppm of rare earth oxide.
5. the preparation method of the described in any item high amplitude magnetic conductivity MnZn Ferrite Materials of Claims 1 to 4, it is characterised in that
Including following preparation step:
A) ingredient: by principal component Fe2O3, ZnO and MnO2It carries out ingredient and is uniformly mixed to obtain mixture；
B) a ball milling: a ball milling material is obtained within ball-milling treatment 2~3 hours after mixture, steel ball and water are mixed；
C) pre-burning: pre-burning after a ball milling material is dried, calcined temperature are 860~950 DEG C, and burn-in time is 1.5~4 hours,
Preburning material is made；
D) secondary ball milling: by addition of C aCO3、Bi2O3It is mixed to get doping material with rare earth oxide and Preburning material, doping is expected,
Steel ball carries out secondary ball milling after mixing with water, the secondary ball milling time 3~5 hours, secondary ball abrasive material is made after dry；
E) be granulated: being added poly-vinyl alcohol solution in secondary ball abrasive material, grinding is granulated or mist projection granulating, it is screened obtain 100~
250 μm of granulation material；
F) it forms: granulation material uniformly being poured into compression moulding in mold and obtains green body；
G) it is sintered: by green body by room temperature to 1300~1400 DEG C of sintering temperature, keeping the temperature 3~6 hours, green body cools down later
To room temperature, high amplitude magnetic conductivity MnZn Ferrite Material is obtained.
6. the preparation method of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 5, it is characterised in that: described
In step b), when ball milling, mixture and water, steel ball quality ratio are 1:(0.9~1.1): (3~6).
7. the preparation method of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 5, it is characterised in that: described
In step d), when ball milling, doping material is 1:(0.9~1.1 with water, steel ball quality ratio): (3~5).
8. the preparation method of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 5, it is characterised in that: described
In step e), the mass concentration of poly-vinyl alcohol solution is 8%~15%, and the additional amount of poly-vinyl alcohol solution is secondary ball abrasive material weight
The 8%~12% of amount.
9. the preparation method of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 5, it is characterised in that: described
In step f), the pressure of compression moulding is 100~200Mpa, 20~60s of dwell time.
10. the preparation method of high amplitude magnetic conductivity MnZn Ferrite Material according to claim 5, it is characterised in that: institute
It states in step g), the temperature rise period for rising to 1100 DEG C from room temperature is air atmosphere, and 1100 DEG C start to be passed through partial pressure of oxygen no more than 5%
Oxygen-nitrogen mixture body, and be passed through oxygen-nitrogen mixture body to the holding stage always and terminate, temperature-fall period is passed through pure nitrogen gas.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116191A (en) * | 2019-12-31 | 2020-05-08 | 天长市中德电子有限公司 | High-permeability low-loss manganese-zinc soft magnetic ferrite material and preparation method thereof |
| CN113213907A (en) * | 2021-06-24 | 2021-08-06 | 横店集团东磁股份有限公司 | Composite ferrite material and preparation method and application thereof |
| CN114031388A (en) * | 2021-11-23 | 2022-02-11 | 山东春光磁电科技有限公司 | Mn-Zn ferrite material and preparation method thereof |
| CN114974774A (en) * | 2022-06-29 | 2022-08-30 | 湖北中烟工业有限责任公司 | Ferrite composite material and preparation method thereof |
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| CN111116191A (en) * | 2019-12-31 | 2020-05-08 | 天长市中德电子有限公司 | High-permeability low-loss manganese-zinc soft magnetic ferrite material and preparation method thereof |
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| CN113213907A (en) * | 2021-06-24 | 2021-08-06 | 横店集团东磁股份有限公司 | Composite ferrite material and preparation method and application thereof |
| CN114031388A (en) * | 2021-11-23 | 2022-02-11 | 山东春光磁电科技有限公司 | Mn-Zn ferrite material and preparation method thereof |
| CN114974774A (en) * | 2022-06-29 | 2022-08-30 | 湖北中烟工业有限责任公司 | Ferrite composite material and preparation method thereof |
| CN114974774B (en) * | 2022-06-29 | 2024-08-27 | 湖北中烟工业有限责任公司 | Ferrite composite material and preparation method thereof |
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